离子色谱法同时测定硫酸氢氯吡格雷中甲酸残留及硫酸盐含量

Simultaneous Determination of Residual Formic Acid and Content of Sulfate in Clopidogrel Bisulfate by Ion Chromatography

  • 摘要: 建立了离子色谱同时测定硫酸氢氯吡格雷原料药中的甲酸残留及硫酸盐含量的方法. 硫酸氢氯吡格雷原料药以2 mmol/L NaOH水溶液超声提取,经过滤后进样分析. 采用Dionex IonPac AS11-HC(4 mm×250 mm)分析柱以及Dionex IonPac AG11-HC(4 mm×50 mm)保护柱,EG 500 KOH在线产生KOH,梯度洗脱,流速1.3 mL/min,柱温30 ℃,进样体积25 μL,抑制电流90 mA. 结果表明,HCOO在0.020 0~1.00 mg/L范围内、SO42−在10.0~40.0 mg/L范围内线性关系良好. HCOO、SO42−检出限分别为10.0、50.0 μg/L,定量限分别为20.0、100 μg/L. 方法前处理简单,灵敏度高,重复性好,适用于硫酸氢氯吡格雷原料药中甲酸残留及硫酸盐含量的同时测定.

     

    Abstract: A method for the simultaneous determination of residual formic acid and the content of sulfate (SO42−) in clopidogrel bisulfate active pharmaceutical ingredient (API) by ion chromatography (IC) was developed. Clopidogrel bisulfate API was sonicated by 2 mmol/L NaOH aqueous solution and then filtered. The analysis was performed on a Dionex IonPac AS11-HC analytical column (4 mm×250 mm) in combination with a Dionex IonPac AG11-HC guard column (4 mm×50 mm). The eluent was KOH produced on-line with an EG 500 KOH in the gradient mode at a flow rate of 1.3 mL/min. The column temperature was kept at 30 ℃ and the injection volume was 25 μL. The suppressor current was 90 mA. The test results showed that good linearity existed over the range of 0.020 0~1.00 mg/L for formic acid, and 10.0~40.0 mg/L for sulfate, respectively. The detection limits (LODs) of formic acid and sulfate were 10.0, 50.0 μg/L, respectively, and the quantification limits (LOQs) were 20.0, 100 μg/L, respectively. The method is simple, highly sensitive, and reproducible, and could be suitable for the detection of residual formic acid and the content of sulfate in clopidogrel bisulfate API.

     

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